Electric Literature of 55304-75-1, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 55304-75-1 as follows.
To a suspension of tert-butyl-1-piperazine carboxylate (27.0 g, 145 mmol) and K2CO3 (40.0 g, 290 mmol) in DMSO (200 ML) were 2,6-dichloro-3-trifluoromethylpyridine (29.1 g, 135 mmol) and toluene (50 ML) added.The thick slurry was stirred at 80 C. for two hours, followed by addition of toluene (0.5 L) and water (1 L).The phases were separated and the organic phase was washed twice with water.The solvent from the dried (MgSO4) organic phase was evaporated at reduced pressure.The solid residue was recrystallized from EtOAc/heptane to give white crystals (37 g).The filtrate from the recrystallization was concentrated and the residue chromatographed on a column of silica with hexane/EtOAc (90:10) to give further 6.0 g of product (total yield 85%).Purity 99% (HPLC); mp 125 C. Anal. (C15H19ClF3N3O2) C, H, N.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,55304-75-1, its application will become more common.
Reference:
Patent; Nilsson, Bjorn M.; Ringberg, Erik; US2003/232814; (2003); A1;,
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